蔬菜中内分泌干扰物4-壬基酚和双酚A的GC-MS检测方法研究

Study on determination of the xenoestrogens 4-nonylphenol and bisphenol A in vegetables using gas chromatography-mass spectrometry

目的 建立蔬菜中内分泌干扰物4-壬基酚（4-NP）和双酚A（BPA）的GC-MS检测方法。方法样品粉碎后，超声波振荡提取，BOND ELUT CH固相萃取小柱净化，二氯甲烷洗脱，无水硫酸钠脱水后BSTFA衍生，GC-MS测定。结果 两种目标化合物线性范围为10～500μg／L（r=0.999），4-NP和BPA的检出限分别为0．1μg／kg和0．02,μg／kg，样品平均加标回收率为85．0％～105．1％，批内、批间精密度均小于10％。结论 该方法具有良好的批内和批问精密度，灵敏度高，适用于蔬菜中痕量4-NP和BPA检测。

To develop a simple and sensitive GC/MS method for the determination of 4-nonylphenol （4-NP） and bisphenol A（BPA） from vegetables. Methods After smashed, the samples were extracted using ultrasonic extraction, and CH cartridge was used to clean the impurity, then desorbed with diehloromethane, the elution was chemically dried with anhydrous sodium sulphate and a silylation step was carried out with N, O-bis（trimethylsilyl） -trifluoroaeetamide （BSTFA） to enhance the selectivity and sensitivity of the detection. Then the derivation were identified and quantified by GC-MS.Results The linear range is from 10 to 500/g/L for two target compounds with the correlation coefficient of 0.999,and the limit of detection（LOD） is 0.1/μg/kg（4-NP） and 0.02/μg/kg （BPA）, respectively. The spiked recoveries of two target compounds are ranged from 85.0% - 105.1%, and the precision are both below 10%. Conclusion This method has fairly high sensitivity and good precision, it can be used to detect the trace amount of 4-NP and BPA from vegetables.